105

ODS STEEL AS A STRUCTURAL MATERIAL FOR

HIGH TEMPERATURE NUCLEAR REACTORS
M.A. Pouchon, M. Döbeli, R. Schelldorfer, J. Chen, W. Hoffelner, C. Degueldre

Oxide-dispersed-strengthened (ODS) ferritic-martensitic steels are examined as possible candidates for

the structural materials to be used in the future generation of High-Temperature Gas-Cooled Nuclear
Reactors, and as a replacement for alternative high-temperature materials for tubing and other structural
components. ODS steels are also being considered as possible material for use in future fusion
applications. Since the oxide particles serve as an interfacial pinning mechanism for moving dislocations,
the creep resistance of the material is improved. However, in order to use such materials in a reactor, their
behaviour under irradiation must be thoroughly examined. In this work, the effects induced by He
implantation are investigated the induced swelling is measured, and the mechanical behaviour of the
irradiated surface is analysed. These first tests are performed at room temperature, for which clear
evidence of swelling and hardening could be observed.

1 INTRODUCTION capabilities in the context of high-temperature gas

Operating temperatures of current Light Water
Reactors (LWRs) do not exceed 350ºC, and the
conversion from thermal to mechanical energy is
accomplished by steam generation and steam
turbines. Suitable materials already exist, and current
research focuses mainly on safety and life
assessment under fuel high-burnup conditions, and on
reactor ageing. In contrast to LWRs, concepts for
future (i.e. Generation IV) nuclear fission plants focus
on the much higher temperatures needed to increase
the thermal-cycle efficiency, and the inclusion of
process-heat applications (e.g. hydrogen production).
Fast neutron spectra are also considered.
1.6
1.4 TRIM profile
1.2
displ. dose [dpa]
turbine applications. Accordingly, the members of the
GIF VHTR and GFR Steering Committees, together
with researchers from FZ Jülich [3] and Petten [4],
have concluded that they should be considered as
serious candidates for future high-temperature nuclear
applications
PM2000 is an ODS alloy of composition 20 wt% Cr,
5.5 wt% Al, 0.5 wt% Ti, 0.5 wt% Y2O3, with Fe
making up the balance. It is manufactured by
mechanically alloying in a high energy mill to produce
a solid solution containing a uniform dispersion of
yttria. The powder is consolidated using hot, isostatic
pressing, followed by hot and cold rolling procedures.
A final thermal treatment completes the production
process [5,6]. The alloy is supplied by Plansee GmbH.
2 EXPERIMENTAL PROCEDURE

fitted prof ile

PM2000 ODS samples are cut and polished in the
1.0 following way. Several samples, of dimensions
3
0.8 6x6x1 mm , are cut in a long, transverse direction.
One surface is then ground with SiC papers, down to
0.6 a P-Grading of 4000. Polishing with a 6 µm and 3 µm
0.4 diamond suspension is then performed, the polishing
being finalized with OP-S (oxide polish suspension)
0.2 for 2 minutes.
0.0 The samples are then irradiated using a 4He beam
++

0.00 1.00
depth [µm]
Fig. 1: Implanted displacement dose profile
calculated by TRIM, and the fit used for
further calculations.
Concepts for nuclear plants are studied world-wide
within the framework of the Generation IV
International Forum (GIF), of which Switzerland is a
full member. The role of ODS materials in fusion
applications has been reviewed by Ukai and Fujiwara
[1] and Hoelzer [2]. Both studies conclude that ODS
materials are interesting for future nuclear
applications. It is worth mentioning that ODS materials
have not yet been considered for High Temperature
Reactors (HTRs), though they have proven
2.00 at ETH Zürich, using a Tandem Accelerator. The main
difference between this procedure and thermal-
neutron irradiation is the high He-to-dpa ratio possible.
However, for this preliminary study, this fact was
accepted, since the data obtained from this
experiment also represents an extreme situation,
which might occur with a fast spectrum. Further
information concerning the simulation of n-irradiation
by charged particles is given in [7].
An even dpa distribution is desirable, so the irradiation
is performed at 4 different incident angles (ranging
from 0° to 66°), at an energy of 1.5 MeV. As a
consequence of this procedure, the damage as a
function of depth is quite uniform: about 0.7 to 1.3 dpa
from 1 to 2.5 µm. Figure 1 shows results from a TRIM
(transport of ions in matter) simulation of the induced
 106
Fig. 2: Surface of the ODS sample, obtained using
AFM. The original data after peak removal is
shown on the left side, and the averaged
profile on the right.
damage profile. The computer code TRIM [8] tends to
underestimate the width of the implantation profile, so
the peaks appear sharper than in reality. The
16 16 16
irradiated fluences are 1.4•10 , 2.8•10 , 5.6•10 and
17 -2
1.12•10 cm . The irradiation is performed through a
Mesh 400 TEM grid covering the sample, the bar
periodicity is 63.5 µm, with a bar width of 30 µm.
Consequently, a bar pattern is produced, which is
used to investigate the sample using Atomic Force
Microscopy (AFM), and thereby derive the swelling
behaviour.
The influence of irradiation is subsequently studied
using a nano-indenter. The samples are examined by
means of atomic-force microscopy, using an
apparatus from Digital Instruments: Dimension 3100.
The maximum scan region obtainable with the AFM
2
head used is 124x124 µm , with a maximum scanning
depth of 6.6 µm. The depth resolution is mainly limited
by noise. The scanning is performed in tapping mode,
in order to reach higher precision and to avoid friction-
related phenomena appearing on the irradiated
surface.
The sample preparation for the PM2000 is rather
difficult, because the dispersed yttria nano-particles
are displaced outwards during ceramographic
preparation, and scratch the surface. Therefore, the
AFM sometimes shows some artificial peaks on the
scan. These are removed using appropriate software,
and the resulting AFM images are then smooth. In all
cases, the swelling is large enough to be well
distinguishable from noise effects and any remaining
artefacts on the scan.
An example of such an analysis is shown in Fig. 2.
The x-direction of the scan is averaged, and a third-
order curve fit is made to the data in the original and
swelled regions.
In order to test the mechanical behaviour, a nano-
indenter, supplied by CSM Instruments SA in
Neuchâtel (Switzerland), is employed. The maximum
load of the apparatus is 500 mN (with a load
resolution of 0.04 µN) and a maximum depth of 20 µm
(with a resolution of 0.04 nm).
Fig. 3: Part of an indent series with 1000 nm
penetration depth. The lighter surface
displaces the non-irradiated part of the
sample, and the darker the irradiated part.
Two measurement series were performed using a
Berkovich tip (a tetrahedral-shaped device with one
vertex sharpened to a point). For both series, the
indent depth is fixed: in the first series at 500 nm, and
in the second at 1 µm. The targeted indent positions
are localized with an optical microscope, connected to
the indenter; positioning is accurate to about 1 µm.
Two series of indents were performed on a sample
irradiated with the dose and damage profile given in
Fig. 1. In each series, the indents were positioned so
that both non-irradiated and irradiated parts of the
sample could be tested. Figure 3 shows part of an
indentation series. The reproducibility of the results is
very good with all load/penetration curves agreeing
with each other in both the irradiated and the non-
irradiated areas.
3 RESULTS
The AFM reveals the swelling pattern of the irradiated
ODS bars, and the degree of swelling is deduced from
the distance between the two curves, resulting in a
displacement dependency as a function of fluence.
The data points of the displacement are shown in Fig.
4; additionally, a bi-linear strain curve is derived from
these data, and displayed in the same Figure.
Because of the limited number of data points, a bi-
linear trend line is chosen to represent the behaviour
rather than a more sophisticated curve. The x-axis
corresponding to the displacement data is the total
fluence; this is an integral measure for the entire
depth. The x-axis for the strain data measures the
displacements per atom, and represents a volume
unit.
The non-linearity of strain as a function of
displacements per atom (dpa), and the fact that the
displacement damage is not constant in the relevant
depth region, imply that the derivation of the strain
data from the total surface displacement is not
straightforward. However, the reverse calculation of
the total displacement at the surface from a given
strain curve and dpa profile is a simple integration.
 107

Displ. dose [dpa]

0.0 0.5 1.0 1.5 2.0
40
Displacement [nm].

30 1.5

20
10 exp. data
trend line
0 0.0
0 5 10
16 -2
Fluence [10 cm ]
Fig. 4: Measured displacement at the sample
surface, and derived strain curve, as functions
of the displacement dose.
Therefore, an initial strain curve is set by assuming a
constant irradiation profile over the relevant depth,
and the curve is then adapted in an iterative way to
meet the experimental surface displacement data.
The hardness is investigated using a nano-indenter,
as described in Section 2. Results are presented for
both the non-irradiated and the irradiated surfaces of
the sample. Figure 5 shows the results of the
indentation tests with an indentation depth of
1000 nm. Two indents are placed on the border line
between the irradiated and the non-irradiated
surfaces, to account for mixed regions. This means
that the abscissa of Fig. 5 not only accounts for the
non-irradiated (0%) and fully-irradiated (100%) data,
but the intermediate data too.
The hardness data are compared to the values
reported in [9], for which the hardness was measured
by a Vickers indenter with a mass of 30 kg and a 2/3"
objective. For the untreated ODS samples, a Vickers
hardness of 326±6 HV30 was reported. Transforming
this into SI units, gives a hardness of 3197±59 MPa,
which agrees well with the value 3207 MPa, the
average of the 3 data points in the non-irradiated (0%)
region in Fig. 5.
4500
Hardness [MPa]
Strain [%]
1.0
Fig. 6: 1000 nm indents into the non-irradiated and
0.5 irradiated surface of the sample. Different
pile-up due to different constrains in plasticity.
15 An important point, which needs to be further clarified,
is the possible influence of the residual stresses
arising from the swelling of the material. The irradiated
volume is enclosed in a non-irradiated environment,
which basically keeps its original dimensions, and
which therefore compresses the irradiated area. The
influence of the stress distribution on the
measurements, already discussed in [10], will be
addressed in later stress analysis calculations.
An important difference in the pile-up behaviour of the
indent border is observed for the irradiated and non-
irradiated regions of the sample seen in Fig. 6.
Whether this difference is due to residual stresses or
to changes in material properties also needs to be
clarified.
4 DISCUSSION
The increased hardness seen for the irradiated
surfaces agrees well with results for ferritic steels
found in the literature. For example, low-activation
ferritic steel has been investigated using the micro-
indentation technique [11] to quantify ion induced
hardening. At an irradiation temperature of 673 K,
irradiation-induced dislocation loops are observed
using TEM, the number and density of the loops
clearly increasing, and their mean size decreasing,
with increasing He concentration.
The irradiation-induced changes in micro-hardness
were no more than 10% at 673 K. In the present
paper, the irradiation-induced hardness changes at
room temperature are 29% for the 1000 nm indents.
The difference may be attributed to the super-imposed
effect of the compressive residual stresses for the
samples investigated here. However, the differences

4000 may be a consequence of the different irradiation

conditions.
3500
In the present study, only effects in the transverse
3000 grain direction have been investigated. Since the
material is anisotropic, the other grain orientations
2500 also need to be studied. Differences in hardness for
the longitudinal and perpendicular extrusion directions
-20 0 20 40 60 80 100 120 have been found in other contexts. These differences
Irradiated surface [%] were mostly found for thermally-treated samples, for
which the hardness generally decreased by up to
Fig. 5: Indent-hardness as a function of the irradiated 23%, and the transversal extrusion direction was 10%
surface to non-irradiated surface ratio of the harder than the longitudinal one. For the untreated
indentation region. samples, the hardness was almost isotropic.
 108
5 CONCLUSIONS [4]
At room temperature, for displacement dose ranges
around 0.7 dpa, PM2000 already displays a major [5]
increase in hardness of 30%, and a strain of around
1%. Annealing at higher temperatures will potentially
decrease the hardening and swelling effects. Future
experimental series will address this issue. A first hint
of a decreased hardness at higher temperatures has
[6]
already been reported [9,11]; the irradiation induced
hardening effect was also reduced at higher
temperatures.
The present work demonstrates that a nano/micro-
[7]
scale approach to characterize materials is valid. In
the case of material hardness, good agreement with
literature data exists, and the swelling-induced
displacements are also as expected.
[8]
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application in nuclear environments”, Journal of
Nuclear Materials, 307, 749-757 (2002).
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Alinger, D.S. Gelles A.F. Rowcliffe, R.L Klueh, [10] S. Suresh, A.E Giannakopoulos, “A new method
B.A. Pint, P.J. Mazias: Advanced Alloy Systems,
Fusion Materials Science peer review, August
27-28, 2001, University of California at Santa
Barbara
[11] Y. Katoh, et al., “The influence of helium co-
http://www.fusionmaterials.pnl.gov/peerreview/ho
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2003.
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